U.S. patent number 11,150,225 [Application Number 15/851,965] was granted by the patent office on 2021-10-19 for filters for liquid flow based devices and systems.
This patent grant is currently assigned to AGILENT TECHNOLOGIES, INC.. The grantee listed for this patent is Agilent Technologies, Inc.. Invention is credited to Qing Bai, Ares Geovanos, Thor Miller Wilbanks, Hongfeng Yin.
United States Patent |
11,150,225 |
Bai , et al. |
October 19, 2021 |
Filters for liquid flow based devices and systems
Abstract
A filter includes an inlet side, an outlet side, and a body. The
body includes a first substrate that includes an array of inlet
holes passing through the first substrate, and a second substrate
that includes an array of outlet holes passing through the second
substrate. The body further includes an intermediate region that
includes a plurality of channels extending along a plane that is
transverse or at an angle to a main axis of the filter. Each
channel communicates directly or indirectly with at least one of
the inlet holes and at least one of the outlet holes. The filter
provides a plurality of fluid flow paths through the body from the
inlet side to the outlet side.
Inventors: |
Bai; Qing (Sunnyvale, CA),
Geovanos; Ares (San Francisco, CA), Yin; Hongfeng
(Cupertino, CA), Wilbanks; Thor Miller (Berkeley, CA) |
Applicant: |
Name |
City |
State |
Country |
Type |
Agilent Technologies, Inc. |
Santa Clara |
CA |
US |
|
|
Assignee: |
AGILENT TECHNOLOGIES, INC.
(Santa Clara, CA)
|
Family
ID: |
1000005873904 |
Appl.
No.: |
15/851,965 |
Filed: |
December 22, 2017 |
Prior Publication Data
|
|
|
|
Document
Identifier |
Publication Date |
|
US 20190195841 A1 |
Jun 27, 2019 |
|
Current U.S.
Class: |
1/1 |
Current CPC
Class: |
G01N
30/603 (20130101); B01D 29/56 (20130101); B01D
29/01 (20130101); B01D 15/22 (20130101); G01N
2030/027 (20130101) |
Current International
Class: |
G01N
30/60 (20060101); B01D 15/22 (20060101); B01D
29/01 (20060101); G01N 30/02 (20060101); B01D
29/56 (20060101) |
References Cited
[Referenced By]
U.S. Patent Documents
Other References
International Search Report and Written Opinion issued in
counterpart PCT Application No. PCT/US2018/056892 dated Jun. 4,
2019. cited by applicant .
Extended European Search Report issued in European Patent
Application No. 18890369.4 dated Aug. 30, 2021, (8 pages). cited by
applicant.
|
Primary Examiner: Mellon; David C
Attorney, Agent or Firm: Mannava & Kang, P.C.
Claims
What is claimed is:
1. A filter, comprising: an inlet side; an outlet side; and a body
having a thickness along a main axis between the inlet side and the
outlet side, and a planar area in a transverse plane orthogonal to
the main axis, the body comprising: a first substrate comprising a
substantially constant thickness and a first outside surface at the
inlet side, a first inside surface, and an array of inlet holes
passing through the first substrate from the first outside surface
to the first inside surface; a second substrate comprising a second
outside surface at the outlet side, a second inside surface facing
the first inside surface, and an array of outlet holes passing
through the second substrate from the second inside surface to the
second outside surface, wherein the outlet holes are not in direct
fluid communication with the inlet holes; and a channel region
comprising a plurality of channels extending in parallel at an
angle to the main axis, each channel of the plurality of channels
communicating with at least one of the inlet holes and at least one
of the outlet holes, wherein: each of the inlet holes directly
communicates with two or more adjacent parallel channels of the
plurality of channels; a channel of the two or more adjacent
parallel channels is disposed adjacent to another channel of the
two or more adjacent parallel channels substantially along a length
of the another channel; the filter comprises a plurality of fluid
flow paths through the body from the inlet side to the outlet side;
and each of the fluid flow paths comprises a first turn between the
at least one of the inlet holes and the two or more adjacent
parallel channels, and a second turn between the two or more
adjacent parallel channels and the at least one of the outlet
holes.
2. The filter of claim 1, wherein the inlet holes and the outlet
holes are parallel with the main axis.
3. The filter of claim 1, wherein the inlet holes, or the outlet
holes, or both the inlet holes and the outlet holes, are
slot-shaped.
4. The filter of claim 1, wherein the plurality of channels extend
along the transverse plane, and the first turn and the second turn
are ninety-degree transitions.
5. The filter of claim 1, wherein the inlet holes are elongated
along a first transverse axis of the transverse plane, and the
channels are elongated along another largest dimension along a
second transverse axis of the transverse plane orthogonal to the
first transverse axis.
6. The filter of claim 1, wherein the outlet holes are elongated
along a first transverse axis of the transverse plane, and the
channels are elongated along a second transverse axis of the
transverse plane orthogonal to the first transverse axis.
7. The filter of claim 1, wherein one or more of the outlet holes
each communicate with two or more of the channels.
8. The filter of claim 1, wherein: the channel region is integral
with the first inside surface; the channel region is integral with
the second inside surface; the channel region is a layer interposed
between the first inside surface and the second inside surface; or
a combination thereof.
9. The filter of claim 1, wherein each channel of the plurality of
channels has a cross-sectional area, and the cross-sectional area
is defined at least in part by a critical dimension that is less
than a minimum size of particles to be blocked by the filter.
10. The filter of claim 9, wherein the cross-sectional area is
defined by a depth along the main axis and a width in the
transverse plane, and the critical dimension is the smaller of the
depth and the width.
11. The filter of claim 1, wherein each channel of the plurality of
channels has a cross-sectional area defined by a depth along the
main axis and a width in the transverse plane, and wherein the
depth is greater than the width or less than the width.
12. The filter of claim 1, wherein the outlet holes are offset from
the inlet holes.
13. The filter of claim 1, wherein the plurality of channels have a
critical dimension in a range from 0.5 .mu.m to 50 .mu.m.
14. A filter, comprising: an inlet plate having a first outside
surface and a first set of holes extending in a first direction to
form oval-shaped oblong openings along the first outside surface;
an outlet plate having a second outside surface and a second set of
holes extending in the first direction to form oblong openings
along the second outside surface, wherein the first set of holes
and the second set of holes are offset from one another, and
wherein the first outside surface and the second outside surface
are oriented as opposite outer surfaces; and a plurality of
parallel channels extending in a second direction, wherein the
plurality of parallel channels is positioned (i) between the inlet
plate and the outlet plate, (ii) on the inlet plate or the outlet
plate, or (iii) in the inlet plate or the outlet plate, and wherein
at least one of the openings along the first outside surface
directly communicates with two or more adjacent parallel channels
of the plurality of parallel channels and at least one of the
openings along the second outside surface directly communicates
with the two or more adjacent parallel channels of the plurality of
parallel channels.
15. A filter comprising: an inlet structure having a first outside
surface and a first set of holes to form non-circular openings
along the first outside surface; an outlet structure having a
second outside surface and a second set of holes to form openings
along the second outside surface, wherein the first set of holes
and the second set of holes are offset from one another, and
wherein the first outside surface and the second outside surface
are oriented as opposite outer surfaces; and a plurality of
channels extending in a direction that is different from a
direction of the first set of holes, wherein the plurality of
channels is contiguously engaged with at least one of the inlet
structure or the outlet structure, and wherein at least one of the
openings along the first outside surface directly communicates with
two or more adjacent channels of the plurality of channels and at
least one of the openings along the second outside surface directly
communicates with the two or more adjacent channels of the
plurality of channels.
16. The filter of claim 15, wherein at least one channel of the
plurality of channels is sloped relative to a plane that includes
the plurality of channels.
17. The filter of claim 15, wherein at least one channel of the
plurality of channels includes a circular cross-section.
18. The filter of claim 15, wherein each channel of the plurality
of channels includes a cross-sectional area that is defined at
least by a dimension that is less than a minimum size of particles
to be blocked by the filter.
Description
TECHNICAL FIELD
The present invention relates generally to filters utilized in
liquid flow-based devices and systems, for example as particulate
filters in flow paths of devices and systems or as frits in liquid
chromatography (LC) columns.
BACKGROUND
Porous filters are utilized in various devices and systems
involving the flow of liquid. Typically, a porous filter is a
planar structure such as a disk or plate. Such a filter generally
has two opposing planar sides, and multiple pores extending through
the thickness of the filter to provide multiple flow paths from one
side to the other side. The filter may be positioned in a liquid
flow path (e.g., the lumen of a liquid conduit) so as to span the
cross-sectional flow area of the flow path. As liquid flows through
the pores of the filter, particles carried in the liquid that are
smaller than the size (cross-sectional dimension) of the pores are
able to pass through the filter, while particles greater than the
pore size are prevented from passing through the filter.
Porous filters are utilized, for example, in liquid chromatography
(LC) systems. In an LC system, a mobile phase consisting of one or
more solvents is driven under a high system pressure through a
sample separation unit, which often is provided in the form of a
chromatography column (or cartridge). In high-performance LC (HPLC)
systems and ultra high-performance LC (UHPLC) systems, the system
pressure may be as high as, for example, 1500 bar or greater. The
LC column contains a stationary phase, which in LC is typically
provided in the form of a packed bed of particles. Porous filters
are utilized in LC columns to retain and stabilize the packed bed
of particles. Specifically, one filter is positioned near the inlet
end (head) of the column, the other filter is positioned near the
outlet end of the column, and the particles are packed between the
two filters. The pore size of the filters is smaller than the size
of the particles. Consequently, the filters prevent the particles
from escaping the column, either through the outlet end as the
mobile phase and sample are driven through the column or through
the inlet end in the event of back flow. When utilized in an LC
column, porous filters are typically referred to as frits.
In certain applications, such as LC applications, the ideal
characteristics of such filters or frits include tight distribution
of desired pore size, high pore density, low back pressure drop,
high operation pressure, and small delay volume. Moreover, there
are increasing demands for high efficiency frits and filters with
very small pore sizes (e.g., below 2 micrometers (.mu.m)) in UHPLC
applications. The most commonly utilized approach to creating
mechanically strong filters/frits of small pore sizes is to sinter
powders or fibers in metals, polymers, and other materials.
However, as the result of such fabrication process, neither the
pore size nor the liquid flow path is well controlled. It is not
uncommon to see particles much larger than the specified pore size
passing through sintered filters/frits. In addition, as the pore
size decreases, it becomes more difficult to make filters/frits
reliably and maintain their pressure drop in a practical range.
FIG. 1A is a scanning electron microscope (SEM) image of a top view
of a region of a sintered stainless steel (SS) frit with the
specification of 0.3 .mu.m porous grade. FIG. 1B is an SEM image of
a cross-sectional view of a region of the sintered SS frit shown in
FIG. 1A. FIG. 2 is a plot of the transmission (filtration)
characteristics of a sintered SS frit such as shown in FIGS. 1A and
1B, specifically the fraction of particles blocked (%) as a
function of particle size (.mu.m). FIG. 2 indicates that 2 .mu.m or
larger particles can pass through the sintered SS frit easily. FIG.
3 is an SEM image of particles collected downstream from an LC
column utilizing such sintered SS frits. FIG. 3 is evidence that a
significant amount of 1.8 .mu.m particles passed through the
sintered SS frit at the outlet end of the column during
operation.
One solution for packing sub-2 .mu.m particles in an LC column
using a 0.3 .mu.m-grade sintered SS frit is to preload the frit
with some larger secondary particles, such as particles with a mean
diameter of 3.5 .mu.m in size and then pack the column with smaller
particles. FIG. 4 is an SEM image of a region of such a frit.
Although this frit can be used to stabilize the column bed, it has
several disadvantages, including high surface area of both the
mechanical frit and the secondary particles, high back pressure,
and potential band broadening in the detected chromatographic peaks
caused by uneven flow through the frit.
In view of the foregoing, an ongoing need exists for improved
filters for liquid flow-based devices and systems, including
filters utilized as frits to retain particulate material.
SUMMARY
To address the foregoing problems, in whole or in part, and/or
other problems that may have been observed by persons skilled in
the art, the present disclosure provides methods, processes,
systems, apparatus, instruments, and/or devices, as described by
way of example in implementations set forth below.
According to one embodiment, a filter includes: an inlet side; an
outlet side; and a body having a thickness along a main axis
between the inlet side and the outlet side, and a planar area in a
transverse plane orthogonal to the main axis, the body comprising:
a first substrate comprising a first outside surface at the inlet
side, a first inside surface, and an array of inlet holes passing
through the first substrate from the first outside surface to the
first inside surface; a second substrate comprising a second
outside surface at the outlet side, a second inside surface facing
the first inside surface, and an array of outlet holes passing
through the second substrate from the second inside surface to the
second outside surface, wherein the outlet holes are not in direct
fluid communication with the inlet holes; and a channel region
comprising a plurality of channels extending at an angle to the
main axis, each channel communicating with at least one of the
inlet holes and at least one of the outlet holes, wherein: the
filter comprises a plurality of fluid flow paths through the body
from the inlet side to the outlet side; each flow path runs from at
least one of the inlet holes to at least one of the channels, and
from the at least one channel to at least one of the outlet holes;
and each flow path comprises a first turn between the at least one
inlet hole and the at least one channel, and a second turn between
the at least one channel and the at least one outlet hole.
According to another embodiment, the first substrate is a first
outer substrate, the second substrate is a second outer substrate,
the channel region is a first channel region, and the channels of
the first channel region are first channels; the filter further
comprises an inner substrate between the first outer substrate and
the second outer substrate, the inner substrate comprising an array
of inner holes passing through the inner substrate, wherein a first
group of the inner holes are in direct fluid communication with
corresponding inlet holes, and a second group of inner holes are in
direct fluid communication with corresponding outlet holes; the
filter further comprises a second channel region comprising a
plurality of second channels extending at an angle to the main
axis; each first channel communicates with at least one of the
inlet holes and at least one of the second group of inner holes;
and each second channel communicates with at least one of the first
group of inner holes and at least one of the outlet holes.
According to another embodiment, the first substrate is a first
outer substrate, the second substrate is a second outer substrate,
the channel region is a first channel region, and the channels of
the first channel region are first channels; the filter further
comprises an inner substrate between the first outer substrate and
the second outer substrate, the inner substrate comprising an array
of inner holes passing through the inner substrate; the filter
further comprises a second channel region comprising a plurality of
second channels extending at an angle to the main axis; each first
channel communicates with at least one of the inlet holes and at
least one of the inner holes; each second channel communicates with
at least one of the inner holes and at least one of the outlet
holes; wherein the inner holes are in direct communication with
neither the inlet holes nor the outlet holes; and the first
channels have a first critical dimension, and the second channels
have a second critical dimension less than the first critical
dimension.
According to another embodiment, the first substrate is a first
outer substrate, the second substrate is a second outer substrate,
the channel region is a first channel region, and the channels of
the first channel region are first channels; the filter further
comprises a first inner substrate and a second inner substrate
stacked between the first outer substrate and the second outer
substrate, the first inner substrate comprising an array of first
inner holes passing through the first inner substrate, and the
second inner substrate comprising an array of second inner holes
passing through the second inner substrate, wherein: the array of
first inner holes comprise a first group of first inner holes and a
second group of first inner holes; the array of second inner holes
comprise a first group of second inner holes and a second group of
second inner holes; the first group of the first inner holes are in
direct fluid communication with corresponding inlet holes, and the
second group of the first inner holes are in fluid communication
with corresponding outlet holes via the second group of second
inner holes, and the first group of second inner holes are in fluid
communication with the inlet holes via the first group of first
inner holes, and the second group of second inner holes are in
direct fluid communication with corresponding outlet holes. The
filter further comprises a second channel region and a third
channel region, the second channel region comprising a plurality of
second channels extending at an angle to the main axis, and the
third channel region comprising a plurality of third channels
extending at an angle to the main axis; each first channel
communicates with at least one of the inlet holes and at least one
of the second group of first inner holes; each second channel
communicates with at least one of the first group of first inner
holes and at least one of the second group of second inner holes;
and each third channel communicates with at least one of the first
group of second inner holes and at least one of the outlet
holes.
According to another embodiment, the first substrate is a first
outer substrate, the second substrate is a second outer substrate,
the channel region is a first channel region, and the channels of
the first channel region are first channels; the filter further
comprises a first inner substrate and a second inner substrate
stacked between the first outer substrate and the second outer
substrate, the first inner substrate comprising an array of first
inner holes passing through the first inner substrate and the
second inner substrate comprising an array of second inner holes
passing through the second inner substrate, wherein the first inner
holes are in direct fluid communication with neither the inlet
holes nor the second inner holes, and the second inner holes are in
direct fluid communication with neither the first inner holes nor
the outlet holes; the filter further comprises a second channel
region and a third channel region, the second channel region
comprising a plurality of second channels extending at an angle to
the main axis, and the third channel region comprising a plurality
of third channels extending at an angle to the main axis; each
first channel communicates with at least one of the inlet holes and
at least one of the first inner holes; each second channel
communicates with at least one of the first inner holes and at
least one of the second inner holes; each third channel
communicates with at least one of the second inner holes and at
least one of the outlet holes; and the first channels have a first
critical dimension, the second channels have a second critical
dimension less than the first critical dimension, and the third
channels have a third critical dimension less than the second
critical dimension.
According to another embodiment, a fluid conduit includes: a
conduit body comprising an inlet end, an outlet end, and a lumen
extending from the inlet end to the outlet end; and a filter
according to any of the embodiments disclosed herein, wherein the
filter is positioned at a location selected from the group
consisting of: the inlet end; the outlet end; and a location in the
lumen between the inlet end and the outlet end.
According to another embodiment, a chromatography column includes:
a column body comprising an inlet end and an outlet end, and an
internal column bore extending from the inlet end to the outlet
end; and a filter according to any of the embodiments disclosed
herein, wherein the filter is positioned at the inlet end or the
outlet end. In an embodiment, one such filter is positioned at the
inlet end, and another such filter is positioned at the outlet end.
In an embodiment, a stationary phase is retained between the two
filters.
Other devices, apparatus, systems, methods, features and advantages
of the invention will be or will become apparent to one with skill
in the art upon examination of the following figures and detailed
description. It is intended that all such additional systems,
methods, features and advantages be included within this
description, be within the scope of the invention, and be protected
by the accompanying claims.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention can be better understood by referring to the
following figures. The components in the figures are not
necessarily to scale, emphasis instead being placed upon
illustrating the principles of the invention. In the figures, like
reference numerals designate corresponding parts throughout the
different views.
FIG. 1A is a scanning electron microscope (SEM) image of a top view
of a region of a conventional sintered stainless steel (SS) frit
with the specification of 0.3 .mu.m porous grade.
FIG. 1B is an SEM image of a cross-sectional view of a region of
the conventional sintered SS frit shown in FIG. 1A.
FIG. 2 is a plot of the transmission (filtration) characteristics
of a conventional sintered SS frit such as shown in FIGS. 1A and
1B.
FIG. 3 is an SEM image of particles collected downstream from an LC
column utilizing conventional sintered SS frits such as shown in
FIGS. 1A and 1B.
FIG. 4 is an SEM image of a region of a conventional frit preloaded
with secondary particles.
FIG. 5A is a perspective view of an example of a filter according
to one embodiment of the present disclosure.
FIG. 5B is a side elevation view of the filter illustrated in FIG.
5A.
FIG. 6A is a top plan view of a first substrate illustrated in FIG.
5A.
FIG. 6B is a cross-sectional side elevation view of the first
substrate illustrated in FIG. 6A, taken along line 6B-6B in FIG.
6A.
FIG. 7A is a top plan view of a second substrate illustrated in
FIG. 5A.
FIG. 7B is a cross-sectional side elevation view of the second
substrate illustrated in FIG. 7A, taken along line 7B-7B in FIG.
7A.
FIG. 8 is an exploded view of the filter illustrated in FIG. 5A, in
which a first substrate and a second substrate are separated from
each other along a main axis C (z-axis).
FIG. 9 is another perspective view of the filter illustrated in
FIG. 5A, specifically from the perspective of a first substrate
thereof.
FIG. 10 is cut-away perspective view a section of the filter
illustrated in FIG. 5A.
FIG. 11A is a scanning electron micrograph (SEM) in image of a
substrate that may be included as part of a body of the filter
illustrated in FIG. 5A.
FIG. 11B is a magnified view of a region of the SEM image of FIG.
11A.
FIG. 12 is a cut-away perspective view of a section of an example
of a filter according to another embodiment.
FIG. 13A is a schematic cross-sectional view of an example of a
horizontal rectangular channel according to an embodiment.
FIG. 13B is a schematic cross-sectional view of an example of a
vertical rectangular channel according to an embodiment.
FIG. 13C is a schematic cross-sectional view of an example of a
T-shaped channel according to an embodiment.
FIG. 13D is a schematic cross-sectional view of an example of a
cross-shaped filter channel according to an embodiment.
FIG. 14 is a schematic cross-sectional view of an example of a
filter according to another embodiment.
FIG. 15 is a schematic cross-sectional view of an example of a
filter according to another embodiment.
FIG. 16 is a plot comparing the transmission (filtration)
characteristics of a conventional sintered SS frit such as shown in
FIGS. 1A and 1B to the transmission (filtration) characteristics of
a filter disclosed herein.
FIG. 17 is a cross-sectional view of an example of a chromatography
column including filters as disclosed herein.
FIG. 18 is a schematic view of an example of a fluidic system that
may include one or more filters as disclosed herein.
DETAILED DESCRIPTION
In the present disclosure, the terms "filter" and "frit" are used
interchangeably, unless specified otherwise or the context dictates
otherwise.
As used herein, the term "fluid" is used in a general sense to
refer to any substance that is flowable through a conduit. Thus,
the term "fluid" may generally refer to a liquid, a gas, or a
supercritical fluid, unless specified otherwise or the context
dictates otherwise.
As used herein, the term "liquid" generally encompasses a liquid
having a single-compound composition, or a mixture of two or more
different liquids such as, for example, two or more different
solvents. A liquid may be a solution, a suspension, a colloid, or
an emulsion. Solid particles and/or gas bubbles may be present in
the liquid.
As used herein, the term "conduit" generally refers to any type of
structure enclosing an interior space that defines a repeatable
path for fluid to flow from one point (e.g., an inlet of the
conduit) to another point (e.g., an outlet of the conduit).
Examples of conduits include, but are not limited to, tubes,
capillaries, ports, chambers, fluidic couplings, etc. The
cross-section (or flow area) of the conduit may be round (e.g.,
circular, elliptical, etc.), polygonal (e.g., square, rectilinear,
etc.), a combination of round and polygonal features.
As used herein, the term "filter passage" generally refers to any
passage defining a fluid flow path through at least a portion of a
filter (or frit) as described herein. Examples of filter passages
include, but are not limited to, holes (e.g., pores, bores, etc.)
and channels. The cross-section (or flow area) of the filter
passage may be round (e.g., circular, elliptical, etc.), polygonal
(e.g., square, rectilinear, etc.), a combination of round and
polygonal features, or a combination of different types of round
features or different types of polygonal features. Examples of
cross-sections having a combination of features include, but are
not limited to, a slot with rounded ends (or a racetrack shape), a
"T" shape, a cross shape, etc.
In some embodiments, the internal bore or lumen of a conduit or
filter passage may have a micro-scale cross-sectional dimension,
i.e. a cross-sectional dimension on the order of micrometers
(.mu.m), for example about 1000 .mu.m (1 mm) or less. Such a
conduit or filter passage may be referred to as a microfluidic (or
micro-scale) conduit or microfluidic (or micro-scale) filter
passage. For example, a microfluidic filter passage may be a
microfluidic hole (or pore) or a microfluidic channel.
As used herein, the term "microfluidic conduit" or "microfluidic
filter passage" also encompasses a conduit or filter passage that
has a nano-scale cross-sectional dimension, i.e. a cross-sectional
dimension on the order of nanometers (nm), for example about 1000
nm (1 .mu.m) or less. Thus, for example, the cross-sectional
dimension of a micro-scale conduit or filter passage may be in a
range from about 100 nm to about 1000 .mu.m.
As used herein, the term "cross-sectional dimension" refers to a
type of dimension that is appropriately descriptive for the shape
of the cross-section of the conduit or filter passage--for example,
diameter in the case of a circular cross-section, major axis in the
case of an elliptical cross-section, or a maximum length (or width
or height) between two opposing sides in the case of a polygonal
cross-section. Additionally, the cross-section of the conduit or
filter passage may have an irregular shape, either deliberately or
as a result of the limitations of fabrication techniques. The
cross-sectional dimension of an irregularly shaped cross-section
may be taken to be the dimension characteristic of a regularly
shaped cross-section that the irregularly shaped cross-section most
closely approximates (e.g., diameter of a circle, major axis of an
ellipse, length of a polygonal side, etc.).
Fluid flow rates through a conduit or filter passage of micro-scale
cross-sectional dimension may be on the order of milliliters per
minute (mL/min), microliters per minute (.mu.L/min), or nanoliters
per minute (nL/min).
As used herein, the term "line" (or "fluid line") may refer to a
single fluidic component that defines a fluid flow path from one
point to another point, or two or more fluidic components that
collectively define a fluid flow path. The fluidic components
making up a given fluid line may be a combination of different
types of fluidic components, wherein adjacent fluidic components
are fluidly coupled to each other. Examples of fluidic components
include, but are not limited to, conduits, filters, chambers, flow
cells, pumps, metering devices, valves, columns, flow controlling
devices, fluid measurement (e.g., flow rate, pressure, temperature,
concentration, etc.) devices, fittings, unions, flow combiners, and
flow splitters.
As used herein, the term "microfluidic device" generally refers to
a device having one or more micro-scale features such as
micro-scale conduits or filter passages.
The present disclosure describes filters (or frits) engineered to
exhibit micro-scale fluid filter passages (e.g., holes and
channels) of highly precise and uniform dimensions. The filters
provide a filtering function, in that particles larger than the
critical dimension of the filter channels (as described below)
cannot pass through the filter. The filtering function may also be
implemented as a retaining function. For example, two filters may
be utilized as frits in a liquid chromatography (LC) column to
retain a packed bed of particles (i.e., a stationary phase) between
the two filters. In such an application, the filters allow a fluid
(e.g., a mobile phase consisting of one or more solvents and a
sample material to be analytically separated by the LC column) to
pass through the LC column while preventing the particles of the
stationary phase from escaping the LC column at either the inlet
end or the outlet end. In LC applications, a goal is to provide a
filter having small filter channels in the range of a few
micrometers or less and offering enough mechanical strength to
withstand the pressures commonly encountered in LC applications.
One or more embodiments of a filter as described herein achieve
such a goal. A filter as described herein may include an
arrangement of filter passages configured to provide a very uniform
flow distribution, which is highly desired in the case of LC
columns as appreciated by persons skilled in the art. A filter as
described herein may include an arrangement of filter passages
configured to provide a high volumetric flow capacity. A filter as
described herein may include graduated sizes of the critical
dimension of the filter channels. For example, the sizes of the
critical dimension may be progressively smaller through the
thickness of the filter as fluid flows from the inlet side to the
outlet side of the filter.
FIG. 5A is a perspective view of an example of a filter 500
according to one embodiment of the present disclosure. FIG. 5B is a
side elevation view of the filter 500. For descriptive purposes,
FIGS. 5A and 5B include a Cartesian (x-y-z) coordinate frame of
reference, the origin of which has been arbitrarily positioned
relative to the filter 500. The z-axis may be referred to herein as
a main axis (or filter axis) C, of the filter 500, which typically
is the central axis of symmetry of the filter 500. The thickness of
the filter 500 is defined along the main axis C. The x-y plane
orthogonal to the z-axis may be referred to herein as the
transverse plane. The transverse cross-sectional area of the filter
500 is defined in the transverse plane. The x-axis may be referred
to herein as the first transverse axis, and the y-axis may be
referred to herein as the second transverse axis.
The filter 500 generally includes an inlet side 504 and an outlet
side 508 axially spaced from the inlet side 504 along the main axis
C. The filter 500 generally includes a body 512 having a planar
geometry. By "planar" is meant that the cross-sectional dimension
of the body 512 (e.g., diameter in the case of a disk) in the
transverse plane is the dominant dimension defining the overall
physical size or footprint of the body 512 (and thus the filter
500), as compared to the typically much smaller thickness of the
body 512. The body 512 provides a plurality of fluid flow paths
through its thickness, as described further below. In use,
unfiltered fluid 516 is received at the inlet side 504 and flows
through the fluid flow paths of the body 512, and resulting
filtered fluid 520 flows out from the outlet side 508.
The body 512 includes a first outside surface 524, and a second
outside surface 528 axially spaced from the first outside surface
524 along the main axis C and parallel to the first outside surface
524. The main axis C is orthogonal to the first outside surface 524
and the second outside surface 528. Thus, the axial distance from
the first outside surface 524 to the second outside surface 528
defines the overall axial thickness of the body 512 (and thus the
filter 500).
In an embodiment, the body 512 includes a first substrate (or
layer) 532 and a second substrate (or layer) 536. The first
substrate 532 includes the first outside surface 524, and the
second substrate 536 includes the second outside surface 528. In
some embodiments, the body 512 may further include one or more
additional, intermediate substrates or layers between the first
substrate 532 and the second substrate 536. Providing multiple
substrates or layers may facilitate fabrication of the filter 500,
and increase the fluid flow capacity (e.g., volumetric fluid flow
rate, mL/min) of the filter 500.
FIG. 6A is a top plan view of the first substrate 532. FIG. 6B is a
cross-sectional side elevation view of the first substrate 532,
taken along line 6B-6B in FIG. 6A. As best shown in a magnified
section 640 of FIG. 6B, the first substrate 532 includes a first
inside surface 644 axially spaced from the first outside surface
524 along the main axis C and parallel to the first outside surface
524. The first substrate 532 further includes an array (or pattern)
of fluid inlet holes 568. The fluid inlet holes 568 are
through-holes that extend through the thickness of the first
substrate 532 from the first outside surface 524 to the first
inside surface 644. In the illustrated embodiment, the inlet holes
568 have an elongated dimension along one axis (x-axis or y-axis)
in the transverse plane. For example, the inlet holes 568 may be
shaped as slots. The slots may have rounded ends (i.e.,
racetrack-shaped, as illustrated) or straight ends (i.e., the slots
may have a rectilinear shape). In other embodiments, the
cross-section of the inlet holes 568 may have a round geometry
(e.g., circular, oval, etc.) or a polygonal geometry.
FIG. 7A is a top plan view of the second substrate 536. FIG. 7B is
a cross-sectional side elevation view of the second substrate 536,
taken along line 7B-7B in FIG. 7A. As best shown in a magnified
section 740 of FIG. 7B, the second substrate 536 includes a second
inside surface 772 axially spaced from the second outside surface
528 along the main axis C and parallel to the second outside
surface 528. In the assembled or fabricated form of the filter 500,
the second inside surface 772 faces the first inside surface 644 of
the first substrate 532 (FIG. 6B). The second substrate 536
includes an array (or pattern) of fluid outlet holes 776. The fluid
outlet holes 776 are through-holes that extend through the
thickness of the second substrate 536 from the second inside
surface 772 to the second outside surface 528. In the illustrated
embodiment, the outlet holes 776 have an elongated dimension along
one axis (x-axis or y-axis) in the transverse plane. For example,
the outlet holes 776 may be shaped as slots. In other embodiments,
the cross-section of the outlet holes 776 may be rounded (e.g.,
circular, oval, etc.) or polygonal.
The configuration of the second substrate 536, including the array
of through-holes, may be generally the same as or similar to the
configuration of the first substrate 532. For example, the inlet
holes 568 and the outlet holes 776 may be elongated along the same
axis in the transverse plane. In the present embodiment, the
positions of the inlet holes 568 in the transverse plane are
spatially (or physically) offset from the positions of the outlet
holes 776 so that the inlet holes 568 and outlet holes 776 are not
in direct fluid communication with each other. As described further
below, the filter 500 includes filter channels in an intermediate
region that provide fluid communication between the inlet holes 568
and the outlet holes 776.
FIG. 8 is an exploded view of the filter 500 in which the first
substrate 532 and the second substrate 536 are separated from each
other along the main axis C (z-axis). As best shown in a magnified
section 840 of FIG. 8, the filter 500 includes an intermediate
channel region or layer 880 between the first substrate 532 and the
second substrate 536. The intermediate region 880 includes a
plurality of filter channels 884 running in a plane at an angle to
the main (C or z) axis (and to the inlet holes 568 and outlet holes
776, which are parallel to the main axis). In one embodiment and as
illustrated, the angle is ninety degrees (90.degree.) to the main
(C or z) axis, i.e., the filter channels 884 are orthogonal
relative to the main (C or z) axis (i.e., in the transverse, or
x-y, plane). This configuration may be desirable for ease of
fabrication and stacking up of multiple layers of filter channels
between the first substrate 532 and the second substrate 536. In
other embodiments, the angle may be less than or greater than
ninety degrees relative to the main axis, i.e., the filter channels
884 may be sloped or tilted relative to the transverse plane. The
array of filter channels 884 is configured such that each channel
884 communicates with at least one of the inlet holes 568 and at
least one of the outlet holes 776. By this configuration, the
filter 500 provides a plurality of fluid flow paths through the
body 512 from the inlet side 504 to the outlet side 508. Each flow
path runs from at least one of the inlet holes 568 to at least one
of the filter channels 884, and from at least one channel 884 to at
least one of the outlet holes 776. Moreover, because the inlet
holes 568 and outlet holes 776 extend along the main axis C
(z-axis) while the filter channels 884 extend at an angle to the
main axis, each flow path includes a (first) angled transition or
turn from the corresponding inlet hole 568 to the corresponding
channel 884, and another (second) angled transition or turn from
the channel 884 to the corresponding outlet hole 776. In the
illustrated embodiment in which the filter channels 884 extend
along the transverse plane orthogonal to the main axis C (z-axis),
each flow path includes a (first) ninety-degree transition from the
corresponding inlet hole 568 to the corresponding channel 884, and
another (second) ninety-degree transition from the channel 884 to
the corresponding outlet hole 776. As illustrated, the filter
channels 884 may extend along the transverse (or other angled)
plane in parallel with each other.
In the embodiment specifically illustrated, the filter channels 884
span a majority of the cross-sectional dimension of the first
substrate 532 and second substrate 536. This configuration enables
each channel 884 to communicate with multiple inlet holes 568 and
multiple outlet holes 776, whereby each channel 884 may be part of
multiple fluid flow paths through the filter 500.
In the embodiment specifically illustrated in which the inlet holes
568 and outlet holes 776 are elongated slots, the filter channels
884 run in a direction in the transverse plane orthogonal to the
direction in the transverse plane along which the inlet holes 568
and outlet holes 776 run. For example, the inlet holes 568 and
outlet holes 776 may run along a first transverse axis (e.g., the
x-axis) while the filter channels 884 run along a second transverse
axis (e.g., the y-axis). This configuration enables each inlet hole
568 and each outlet hole 776 to communicate with multiple filter
channels 884.
FIG. 9 is another perspective view of the filter 500, specifically
from the perspective of the first substrate 532. In the present
embodiment, as best shown in a magnified section 940 of FIG. 9,
each inlet hole 568 when provided as an elongated slot may
communicate with multiple filter channels 884 (three channels 884
in the illustrated example). Hence, a fluid flow path running
through a given inlet hole 568, upon transitioning to the
intermediate region 880, may be split into multiple flow paths
through multiple respective filter channels 884. Moreover, the
fluid entering a given channel 884 from a corresponding inlet hole
568 may be split into two flow paths running in opposite directions
along that channel 884.
FIG. 9 may also be representative of a perspective view of the
filter 500 from the perspective of the second substrate 536. In the
present embodiment, multiple filter channels 884 (three channels
884 in the illustrated example) may communicate with a single
outlet hole 776, whereby multiple fluid flow paths merge at each
outlet hole 776.
FIG. 10 is a cut-away perspective view of a section of the filter
500. As shown in FIG. 10, the outlet holes 776 are not in direct
fluid communication with the inlet holes 568. Instead, the outlet
holes 776 fluidly communicate with the inlet holes 568 via the
intervening filter channels 884. In the context of the present
disclosure, the feature "not in direct fluid communication" means
that the outlet holes 776 do not have a direct line of sight along
the main axis C with the inlet holes 568. In the present
embodiment, the feature "not in direct fluid communication" is
realized by the offset positioning of the inlet holes 568 above the
filter channels 884 relative to the outlet holes 776 below the
filter channels 884. In other words, the inlet holes 568 and the
outlet holes 776 are not aligned with each other. The feature "not
in direct fluid communication" may also be characterized by the
fluid flow paths from the inlet holes 568 to the outlet holes 776
including at least two turns. Thus in the present embodiment, a
given flow path passes through an inlet hole 568 along (or parallel
to) the main axis, then turns into a channel 884 and passes through
the channel 884 at an angle to the main axis, then turns into an
outlet hole 776 and passes through the outlet hole 776 along (or
parallel to) the main axis.
The inlet holes 568, the outlet holes 776, and the filter channels
884 each have a depth defined along the main axis C (z-axis). The
depth of the filter channels 884 is designated d in FIG. 10. When
configured as slots, the inlet holes 568 and the outlet holes 776
have a length (elongated dimension) along an axis (e.g., the first
transverse axis, or x-axis) in the transverse plane. The filter
channels 884 have a length (elongated dimension) along an axis
(e.g., the second transverse axis, or y-axis) in the transverse
plane, and a width w along an axis (e.g., the first transverse
axis, or x-axis) orthogonal to the length. In the present
embodiment, the filter channels 884 may be characterized as
"horizontal" in that their width w in the transverse plane is
significantly (or predominantly, or appreciably) greater than their
depth d along (parallel to) the main (z) axis. In the present
context, the term "significantly" means that the filter channels
884 are observed (as may be aided by microscopic imaging) to be
horizontally oriented in the manner described in this paragraph. In
one non-exclusive example, the width w of the filter channels 884
is two times or more greater than their depth d. In the case of
horizontal filter channels 884 as illustrated, the depth of the
filter channels 884 is less than the minimum particle size, i.e.,
the minimum size of the particles intended to be retained and not
passed through the filter 500. That is, the depth of the filter
channels 884 is the critical dimension (described further below) of
the embodiment of the filter 500 shown in FIG. 10. In one
embodiment in which the inlet holes 568 and the outlet holes 776
are configured as slots, the slot length of the inlet holes 568 and
the outlet holes 776 is greater than the width of the filter
channels 884, as described above.
In one non-exclusive example, the inlet holes 568, the outlet holes
776, and the filter channels 884 have the following dimensions. The
inlet holes 568 and the outlet holes 776 have a depth in a range
from 10 to 1000 .mu.m. The inlet holes 568 and the outlet holes 776
may have a cross-sectional dimension (e.g., diameter) in a range
from 20 to 200 .mu.m. When configured as slots, the inlet holes 568
and the outlet holes 776 have a length in a range from 50 to 500
.mu.m. The filter channels 884 have a depth in a range from 0.5 to
50 .mu.m, a length in a range from 5 to 100 .mu.m, and a width in a
range from 0.5 to 100 .mu.m.
In an embodiment, the inlet holes 568 are uniformly spaced from
each other in the transverse plane, the outlet holes 776 are
uniformly spaced from each other in the transverse plane, and the
filter channels 884 are uniformly spaced from each other in the
transverse plane.
As described above, the filter 500 may be characterized as
including an intermediate region 880 "between" the first substrate
532 and the second substrate 536. The intermediate region 880 is
the portion of the filter 500 that includes a plurality of filter
channels 884. In one embodiment, the intermediate region 880 is
integral with the first substrate 532. For example, the filter
channels 884 of the intermediate region 880 may be formed on the
first inside surface 644 of the first substrate 532. In another
embodiment, the intermediate region 880 is integral with the second
substrate 536. For example, the filter channels 884 may be formed
on the second inside surface 772 of the second substrate 536.
FIG. 11A is a scanning electron micrograph (SEM) in image of a
substrate and intermediate region (where the channels are located
or formed) that may be included as part of the body 512 of the
filter 500. FIG. 11B is a magnified view of a region of the SEM
image of FIG. 11A. As shown, the channels 884 are provided as
recesses on either the first inside surface 644 of the first
substrate 532 or the second inside surface 772 of the second
substrate 536.
In another embodiment, the intermediate region 880 is a distinct
layer fabricated separately from and positioned between the first
substrate 532 and the second substrate 536. In this case, the
intermediate region 880 may be properly aligned with and positioned
on either the first inside surface 644 of the first substrate 532
or the second inside surface 772 of the second substrate 536 before
attaching the first substrate 532 and the second substrate 536
together.
FIG. 12 is a cut-away perspective view of a section of an example
of a filter 1200 according to another embodiment. The filter 1200
includes an intermediate channel region 1280 that includes a
plurality of filter channels 1284 providing fluidic connections
between inlet holes 568 and outlet holes 776 as described elsewhere
herein. In the present embodiment, and in comparison to the
horizontal filter channels 884 described above in conjunction with
FIG. 10, the filter channels 1284 of the filter 1200 may be
characterized as "vertical" in that their depth d along (parallel
to) the main (z) axis is significantly (or predominantly, or
appreciably) greater than their width w in the transverse plane. In
the present context, the term "significantly" means that the filter
channels 1284 are observed (as may be aided by microscopic imaging)
to be vertically oriented in the manner described in this
paragraph. In one non-exclusive example, the depth d of the filter
channels 884 is two times or more greater than their width w. In
the case of vertical filter channels 1284, the width of the filter
channels 1284 is less than the minimum particle size to be retained
by the filter 1200. That is, the width of the filter channels 1284
is the critical dimension (described further below) of the filter
1200. The filter 1200 may otherwise be similar to the filter 500
having horizontal filter channels 884 described above in
conjunction with FIGS. 5A to 11B, and may be fabricated utilizing
the same techniques described herein.
As in the embodiment described above and illustrated in FIGS.
5A-10, the outlet holes 776 of the filter 1200 are not in direct
fluid communication with the inlet holes 568, but instead are
fluidly interconnected by the filter channels 1284. That is, there
is no direct line of sight along the main axis C between the inlet
holes 568 and the outlet holes 776. In the present embodiment, this
feature is again implemented by the outlet holes 776 being
spatially (or physically) offset from (i.e., not aligned with) the
inlet holes 568. Each fluid flow path includes at least two turns,
for example into and out from an interconnecting filter channel
1284.
FIGS. 13A-13D are schematic cross-sectional views of examples of
channels that may be disposed in the intermediate region of a
filter as described herein, and fluidly interconnect inlet holes
and outlet holes of the filter. In each of FIGS. 13A-13D, the
direction of fluid flow through the channel is into or out from the
plane of the drawing sheet, i.e., along a transverse axis relative
to the fluid flow through the inlet and outlet holes that is
parallel to the main axis of the filter. In each embodiment, the
channel has a critical dimension, which dimension is smaller than
the size of the particle to be retained. Thus, the critical
dimension determines whether a particle of a certain size can pass
through the channel and hence through the filter. The critical
dimension depends on the cross-sectional geometry of the
channel.
FIG. 13A illustrates a horizontally oriented rectangular channel
1384A, as described above in conjunction with FIG. 10. The channel
1384A has a critical dimension 1388A, as indicated by arrows. In
this case, the critical dimension 1388A is the depth of the channel
1384A, i.e., the dimension along the vertical direction from the
perspective of FIG. 13A.
FIG. 13B illustrates a vertically oriented rectangular channel
1384C, as described above in conjunction with FIG. 12. The channel
1384B has a critical dimension 1388B, as indicated by arrows. In
this case, the critical dimension 1388B is the width of the channel
1384B, i.e., the dimension along the horizontal direction from the
perspective of FIG. 13B.
FIG. 13C illustrates a T-shaped channel 1384C defined by a vertical
section 1392C and a horizontal section 1396C. The channel 1384C has
a critical dimension 1388C, as indicated by arrows. In this case,
the critical dimension 1388C is the width (in the horizontal
direction) of the vertical section 1392C. This assumes that the
depth (in the vertical direction) of the horizontal section 1396C
is not larger than the width of the vertical section 1392C. If the
depth of the horizontal section 1396C were larger than the width of
the vertical section 1392C, then the critical dimension would be
the size of the depth of the horizontal section 1396C.
FIG. 13D illustrates a cross-shaped channel 1384D defined by a
horizontal section 1396D intersected by one or more vertical
sections 1392D. Each intersection thus has a square-shaped
cross-section. The channel 1384D has a critical dimension 1388D, as
indicated by arrows. In this case, the critical dimension 1388D is
the diagonal between opposing corners of the square-shaped
cross-section of each intersection.
Similarly, in an embodiment where a filter channel has a simple
square-shaped cross-section (without horizontal and vertical
extensions as in the cross-shaped channel 1384D illustrated in FIG.
13D), the critical dimension would be the diagonal between opposing
corners of the square-shaped cross-section. Alternatively, a filter
channel may have a circular cross-section, in which case the
critical dimension would be the diameter of the cross-section.
Generally, the components of the filter 500 (or 1200) may be
composed of one or more materials effective for withstanding high
fluid pressure regimes as described herein, e.g., in a range of 100
bar or greater, and capable of being engineered to produce
high-resolution features such as through-holes and channels as
described herein. Examples of such materials include various
metals, metal alloys, metalloids (e.g., silicon), ceramics (e.g.,
glasses), and polymers. A few specific examples include, but are
not limited to, stainless steel (SS), titanium, palladium and a
nickel-cobalt (NiCo) alloy such as an 80% nickel/20% cobalt alloy.
Metals such as palladium are useful for bio-compatible
applications.
Generally, the filter 500 may be fabricated by any process suitable
for accurately creating high-resolution features on the small
scales noted above using materials capable of withstanding the high
pressures noted above. Microfabrication processes may be utilized
entailing material-additive process steps (e.g., chemical vapor
deposition, physical vapor deposition, electro-deposition,
electro-plating, diffusion bonding, selective fusing, etc.),
material-subtractive process steps (e.g., wet (chemical) etching,
electro-chemical machining, dry etching (e.g., plasma etching, deep
reactive ion etching (DRIE), laser milling, etc.), stamping, or a
combination of the foregoing, such as the type of processes
utilized in fields of microfluidics, microelectronics, and
micro-electromechanical systems (MEMS). In one non-limiting
example, the filter 500 is fabricated by an additive process that
utilizes photolithography techniques in combination with
electrodeposition of metals. In some embodiments, multiple filters
500 may be fabricated simultaneously as dies on a single substrate
(e.g., a 4-inch wafer) and thereafter singulated from the
substrate. In some embodiments, the surfaces of the filter 500
(particularly the surfaces exposed to the fluid flow, i.e., the
surfaces defining holes and channels) may be deactivated as part of
the fabrication process, such as by applying a suitable coating or
surface treatment/functionalization that renders the holes and
channels chemically inert and/or of low absorptivity to the fluid.
Moreover, the surfaces may be treated or functionalized so as to
impart or enhance a property such as, for example, anti-stiction,
hydrophobicity, hydrophilicity, lipophobicity, lipophilicity, low
absorptivity, etc., as needed or desirable for a particular
application. Coatings and surface treatments/functionalizations for
all such purposes are readily appreciated by persons skilled in the
art.
In some embodiments, the filter 500 may be fabricated utilizing a
layer-by-layer metal deposition technique in which internal
features (e.g., the filter channels 884) are formed by depositing
metal through appropriately patterned photolithographic masks. In
such embodiments, the filter 500 may include a plurality of
material layers stacked along the main axis C, such as two outer
substrates 532 and 536 and one or more intermediate layers between
the two outer substrates 532 and 536. In some embodiments, before
or after a given layer has been deposited, additional material may
be deposited on that layer and in the negative space to provide a
supporting structure for the subsequent layer or layers to be
deposited. At a later stage of the fabrication, the additional
material may be removed from the negative space by an appropriate
etching technique or other material removal technique. In some
embodiments, features such as through-holes and/or channels may be
formed on or in the substrates, and the substrates are thereafter
appropriately aligned with each other and attached together.
Attachment may entail, for example, bonding (e.g., thermal
compression, adhesive, eutectic, anodic, surface activated bonding,
etc.), welding, gluing, etc. In some embodiments, an
adhesion-promoting layer may be applied to a surface of a substrate
or layer prior to attaching another substrate or layer to the first
substrate or layer.
FIG. 14 is a schematic cross-sectional view of an example of a
filter 1400 according to another embodiment. The filter 1400 may be
a multi-stage configuration derived from the basic filter
configurations described above in conjunction with FIGS. 5A to
13D.
The filter 1400 includes first (outer) substrate (or layer) 1432
having an array of inlet holes 1468 and a second (outer) substrate
(or layer) 1436 having an array of outlet holes 1476. The filter
1400 further includes one or more additional, inner substrates (or
layers) between the first (outer) substrate 1432 and the second
(outer) substrate 1436 to provide high fluid flow capacity. In the
illustrated embodiment, the filter 1400 includes two inner
substrates, namely a first inner substrate 1406 and a second inner
substrate 1410. The first inner substrate 1406 includes an array or
pattern of first inner holes 1414 running through its thickness,
and the second inner substrate 1410 includes an array or pattern of
second inner holes 1418 running through its thickness. The first
inner holes 1414 and second inner holes 1418 are arranged to be
part of the plurality of fluid flow paths (e.g., via filter
channels) from the of inlet holes 1468 to the outlet holes 1476.
Fluid flow through the first inner holes 1414 and the second inner
holes 1418, as well as the inlet holes 1468 and the outlet holes
1476, is parallel to the main axis of the filter 1400 as depicted
by vertical arrows.
In an embodiment, the number of first inner holes 1414 is greater
than either the number of inlet holes 1468 or the number of outlet
holes 1476. Likewise, the number of second inner holes 1418 is
greater than either the number of inlet holes 1468 or the number of
outlet holes 1476. The pattern and number of second inner holes
1418 may be the same as the pattern and number of first inner holes
1414. Corresponding pairs of first inner holes 1414 and second
inner holes 1418 may be in direct fluid communication (i.e. in
direct line of sight, e.g. aligned) with each other. In an
embodiment, the pattern of first inner holes 1414 (and likewise the
pattern of second inner holes 1418) may be a combination of the
pattern of inlet holes 1468 and the pattern of outlet holes
1476.
In the illustrated embodiment, some (i.e., a first group) of the
first inner holes 1414 are in direct fluid communication (i.e. in
direct line of sight, e.g. aligned) with corresponding inlet holes
1468 to receive the fluid exiting the first substrate 1432, while
the other (i.e., a second group of) first inner holes 1414 are in
fluid communication with corresponding outlet holes 1476 via a
second group of second inner holes 1418 (and spatially offset from
the inlet holes 1468). Also, the first inner holes 1414 and the
second inner holes 1418 are in direct fluid communication with each
other. Thus, some (i.e., a first group) of the second inner holes
1418 are in fluid communication with the inlet holes 1468 via the
first group of first inner holes 1414 (and spatially offset from
the outlet holes 1476), while the other (i.e., a second group of)
second inner holes 1418 are in direct fluid communication with the
outlet holes 1476 (and spatially offset from the inlet holes
1468).
As in other embodiments, the filter 1400 includes filter channels
that provide fluid communication between the inlet holes 1468 and
the outlet holes 1476 via transverse (relative to the main axis)
fluid pathways through the filter channels. Depending on the
elevational locations of the filter channels relative to the main
axis, one or more sets of filter channels may receive fluid from
the inlet holes 1468 via the first inner holes 1414 or the second
inner holes 1418 and may provide fluid to the outlet holes 1476 via
the first inner holes 1414 or the second inner holes 1418. In the
illustrated embodiment, a first intermediate channel region (or
layer) 1422 is disposed between the first (outer) substrate 1432
and the first inner substrate 1406, a second intermediate channel
region (or layer) 1426 is disposed between the first inner
substrate 1406 and the second inner substrate 1410, and a third
intermediate channel region (or layer) 1430 is disposed between the
second inner substrate 1410 and the second (outer) substrate 1436.
The first intermediate channel region 1422, the second intermediate
channel region 1426, and the third intermediate channel region 1430
each include a plurality of filter channels. Fluid flow through the
filter channels is transverse (or, as described above, at some
other angle) to the main axis of the filter 1400, as depicted by
horizontal arrows. The network of fluid flow paths--defined by the
inlet holes 1468, first inner holes 1414, second inner holes 1418,
outlet holes 1476, and filter channels--is configured such that all
fluid entering an inlet hole 1468 must pass through at least one
filter channel before exiting one of the outlet holes 1476. The
filter channels may be configured according to any of the
embodiments described herein, such as illustrated in FIGS. 8-13D.
The filter channels may be formed by material-additive and/or
material-subtractive processes as described herein.
In other embodiments, the filter 1400 may include only one inner
substrate between the first outer substrate 1432 and the second
outer substrate 1436. In such embodiments, the filter 1400 may
generally have the same configuration as that shown in FIG. 14. As
an example, the single inner substrate has an array of inner holes
passing through the inner substrate as described above. A first
group of the inner holes are in direct fluid communication with
corresponding inlet holes 1468, and a second group of inner holes
are in direct fluid communication with corresponding outlet holes
1476. The filter 1400 has a first channel region between the first
outer substrate 1432 and the inner substrate, and a second channel
region between the inner substrate and the second outer substrate
1436. The first channel region includes a plurality of first
channels extending in a plane at an angle to the main axis of the
filter 1400, and the second channel region includes a plurality of
second channels extending in a plane at an angle to the main axis.
Each first channel communicates with at least one of the inlet
holes 1468 and at least one of the inner holes, and each second
channel communicates with at least one of the inner holes and at
least one of the outlet holes 1476.
In other embodiments, the filter 1400 may include more than two
inner substrates, thereby further increasing the capacity of the
filter 1400.
High capacity filters are highly desirable because of their high
porosity (without sacrificing pore dimensions or active area), low
operation pressure and high clogging resistance. However, the
capacity of conventional sintered stainless steel (SS) frits is
very limited and decreases as the pore size decreases. On the other
hand, the capacity of an engineered filter as disclosed herein may
be increased multiple times by utilizing the configuration
described above in conjunction with FIG. 14. For example, when an
inner substrate (e.g., first inner substrate 1406 or second inner
substrate 1410)--having a pattern of through-holes that is the
combined pattern of inlet holes 1468 and outlet holes 1476, and
having similar filter channels--is added between the two outer
substrates (e.g., first substrate 1432 and second substrate 1436),
the capacity of the filter doubles in comparison to the basic
two-substrate filter design. This increased capacity is due to the
addition of more filter channels in the network of fluid paths
between the inlet and outlet holes of the two outer substrates.
Further, when two stacked inner substrates (e.g., both the first
inner substrate 1406 and second inner substrate 1410) having
similar through-hole patterns and filter channels are added between
the two outer substrates (as shown in FIG. 14), the capacity of the
filter triples due to the addition of even more filter channels.
Each time an additional substrate is added between the two outer
substrates of the filter, the capacity of the filter is increased
accordingly because of the added filter channels, which is achieved
without increasing the active working area of the filter.
FIG. 15 is a schematic cross-sectional view of an example of a
filter 1500 according to another embodiment. The filter 1500 is
another example of a multi-stage configuration.
The filter 1500 includes first (outer) substrate (or layer) 1532
having an array of inlet holes 1568 and a second (outer) substrate
(or layer) 1536 having an array of outlet holes 1576. The filter
1500 further includes one or more additional, inner substrates (or
layers) between the first (outer) substrate 1532 and the second
(outer) substrate 1536. In the illustrated embodiment, the filter
1500 includes two inner substrates, namely a first inner substrate
1506 and a second inner substrate 1510. The first inner substrate
1506 includes an array or pattern of first inner holes 1514 running
through its thickness, and the second inner substrate 1510 includes
an array or pattern of second inner holes 1518 running through its
thickness. The first inner holes 1514 and second inner holes 1518
are arranged to be part of the plurality of fluid flow paths (e.g.,
via filter channels) from the inlet holes 1568 to the outlet holes
1576. Fluid flow through the first inner holes 1514 and the second
inner holes 1518, as well as the inlet holes 1568 and the outlet
holes 1576, is parallel to the main axis of the filter 1500 as
depicted by vertical arrows.
As in other embodiments, the filter 1500 includes filter channels
that provide fluid communication between the inlet holes 1568 and
the outlet holes 1576 via transverse (relative to the main axis)
fluid pathways through the filter channels. In the illustrated
embodiment, a first intermediate channel region (or layer) 1522 is
disposed between the first (outer) substrate 1532 and the first
inner substrate 1506, a second intermediate channel region (or
layer) 1526 is disposed between the first inner substrate 1506 and
the second inner substrate 1510, and a third intermediate channel
region (or layer) 1530 is disposed between the second (outer)
substrate 1536 and the second inner substrate 1510. The first
intermediate channel region 1522, the second intermediate channel
region 1526, and the third intermediate channel region 1530 each
include a plurality of filter channels. Fluid flow through the
filter channels is transverse (or, as described above, at some
other angle) to the main axis of the filter 1500, as depicted by
horizontal arrows. The network of fluid flow paths--defined by the
inlet holes 1568, first inner holes 1514, second inner holes 1518,
outlet holes 1576, and filter channels--is configured such that all
fluid entering an inlet hole 1568 must pass through at least one
filter channel in each of the three intermediate channel regions
1522, 1526, and 1530 sequentially before exiting one of the outlet
holes 1576. The filter channels may be configured according to any
of the embodiments described herein, such as illustrated in FIGS.
8-13D. The filter channels may be formed by material-additive
and/or material-subtractive processes as described herein.
In an embodiment and as illustrated, the critical dimension
(described above) of the filter channels is graduated, such that
the critical dimension decreases at each successive intermediate
channel region 1522, 1526, and 1530 along the main axis in the
axial direction of fluid flow. In this configuration, the filter
channels closest to the inlet side of the filter 1500 have the
largest critical dimension, the filter channels closest to the
outlet side of the filter 1500 have the smallest critical
dimension, and intermediate levels of filter channels have
respective critical dimensions that are successively reduced
between largest critical dimension and the smallest critical
dimension. For example, in the embodiment specifically illustrated
in FIG. 15, the filter channels of the first intermediate channel
region 1522 have a first critical dimension, which is the largest
critical dimension provided by the filter 1500. The filter channels
of the second intermediate channel region 1526 have a second
critical dimension, which is less than the first critical
dimension. The filter channels of the third intermediate channel
region 1530 have a third critical dimension, which is less than the
second critical dimension. Because in the present example the third
intermediate channel region 1530 is the final channel region
(closest to the outlet side of the filter 1500), the filter
channels of the third intermediate channel region 1530 have the
smallest critical dimension provided by the filter 1500.
With the graduated configuration, the filter 1500 provides a series
of incrementally decreasing particle cut sizes. This configuration
is useful for improving the clogging resistance of the filter 1500.
By this configuration, any large, undesirable particles can be
blocked first by larger filter channels, preventing them reaching
to the smaller filter channels, which can be more easily
clogged.
In other embodiments, the filter 1500 may include only one inner
substrate between the first outer substrate 1532 and the second
outer substrate 1536. In such embodiments, the filter 1500 may
generally have the same configuration as that shown in FIG. 15. As
an example, the single inner substrate has an array of inner holes
passing through the inner substrate as described above. The filter
1500 has a first channel region between the first outer substrate
1532 and the inner substrate, and a second channel region between
the inner substrate and the second outer substrate 1536. The first
channel region includes a plurality of first channels extending in
a plane at an angle to the main axis of the filter 1500, and the
second channel region includes a plurality of second channels
extending in a plane at an angle to the main axis. Each first
channel communicates with at least one of the inlet holes 1568 and
at least one of the inner holes, and each second channel
communicates with at least one of the inner holes and at least one
of the outlet holes 1576. The first channels have a first critical
dimension, and the second channels have a second critical dimension
less than the first critical dimension.
As another example, in an embodiment in which a single inner
substrate is interposed between the first outer substrate 1532 and
the second outer substrate 1536, the inner holes of the inner
substrate may be spatially offset from both the inlet holes 1568
and the outlet holes 1576.
In other embodiments, the filter 1500 may include more than two
inner substrates, thereby providing additional graduations in the
critical dimension.
As in other embodiments, the outlet holes 1576 are not in direct
fluid communication with the inlet holes 1568. This is due not only
to the presence of the intervening filter channels, but also the
presence of intermediate layers (e.g., first inner substrate 1506
and second inner substrate 1510). In the present embodiment, it is
also convenient for the inlet holes 1568 and outlet holes 1576 to
be spatially offset from (not aligned with) each other because of
the use of two hole patterns and the even number of intervening
layers. Further, in the present embodiment and as illustrated, the
first inner holes 1514 are offset from the inlet holes 1568 and
from the second inner holes 1518. Also, the second inner holes
1518, in addition to being offset from the first inner holes 1514,
are offset from the outlet holes 1576. Thus, in this embodiment,
the first inner holes 1514 are in direct fluid communication with
neither the inlet holes 1568 nor the second inner holes 1518, and
the second inner holes 1518 are in direct fluid communication with
neither the first inner holes 1514 nor the outlet holes 1576.
Generally, in embodiments where the fluid flows sequentially
through multiple groups of filter channels, the holes of a given
substrate may be offset from the holes of (each) adjacent
substrate.
On the other hand, in other embodiments that contain an odd number
of stacked substrates (e.g., 3, 5, etc.), the inlet holes 1568 and
the outlet holes 1576 may be aligned with each other, but
nonetheless are not in direct fluid communication with each other
due to the intervening filter channels and one or more intermediate
layers.
Generally, the inner holes of a given inner substrate may be offset
from the inlet holes 1568, or from the outlet holes 1576, or from
both the inlet holes 1568 and the outlet holes 1576, depending on
the position of that inner substrate in the stack and how many
substrates are provided in the filter.
FIG. 16 illustrates plots comparing the transmission (filtration)
characteristics of a conventional sintered SS frit, 0.3 .mu.m grade
(dotted line) such as shown in FIGS. 1A and 1B to the transmission
(filtration) characteristics of a filter disclosed herein (solid
line), namely the filter 500 described above and illustrated in
FIGS. 5A-11B. The filter channels of the filter disclosed herein
had a critical dimension of less than 1.0 .mu.m. Specifically, FIG.
16 illustrates plots of the fraction of particles blocked (%) as a
function of particle size (.mu.m). The same fluid sample was run
through both the conventional SS frit and the filter disclosed
herein. FIG. 16 demonstrates that the filter disclosed herein has a
narrow distribution of pore sizes that are smaller than 1 .mu.m,
and therefore shows a sharp particle cutoff curve that allowed 100%
of the particles in the fluid smaller than 0.75 .mu.m to pass
through while blocking 100% of the particles larger than 1 .mu.m.
By comparison, the conventional SS frit has a significantly wider
particle retaining range of from 0.75 .mu.m to over 2 .mu.m.
Although specified as 0.3 .mu.m grade, an extrapolated number from
a bubble test and not a physical measurement, the conventional SS
frit has a large range of pore sizes, with the maximum pore size
being well over 2 .mu.m.
A filter as described herein may be mounted to or integrated with a
variety of fluidic components such as, for example, capillary
tubes, fluidic fittings, chromatographic columns (or cartridges),
microfluidic chips, and the like. In addition to columns or
cartridges utilized in LC applications, the filter 500 may be
mounted to or integrated with columns utilized in supercritical
fluid chromatography (SFC) and extraction cells utilized in
supercritical fluid extraction (SFE). A filter as described herein
may be provided in a variety of liquid flow-based systems, with
chromatography systems being just one example.
FIG. 17 is a cross-sectional view of an example of a chromatography
column 1700 that includes filters as disclosed herein. The column
1700 generally extends along a central (or longitudinal) axis 1702
from a first column end 1704 to a second column end 1706. The
features of the column 1700 may be the same at the first column end
1704 and the second column end 1706, in which case the designation
of which column end 1704 or 1706 serves as the inlet end or the
outlet end is arbitrary. The column 1700 generally includes a
column wall 1710 elongated along the axis 1702 that encloses a
column interior 1712. The wall 1710 is typically cylindrical (e.g.,
a tube) and thus the column interior 1712 is typically a
cylindrical bore between the column ends 1704 and 1706. The column
1700 includes components at the column ends 1704 and 1706 for
providing fluidic interfaces between the column interior 1712 and
tubing or other fluidic components external to the column 1700. For
example, the column 1700 may include a first end fitting 1714
securely engaging the wall 1710 at the first column end 1704, and a
second end fitting 1718 securely engaging the wall 1710 at the
second column end 1706. In the present context, "securely engaging"
generally means that the end fittings 1714 and 1718 will not become
disengaged from the wall 1710 during normal, intended operations of
the column 1700, including at the pressures typically contemplated
for the specific type of chromatography being performed (e.g.,
HPLC, UHPLC, SFC, etc.) and at the generally higher pressures
applied during the packing of stationary phase media into the
column 1700. The end fittings 1714 and 1718 may be securely engaged
to the wall 1710 via the mating of complementary threads (not
shown) on inside surfaces of the end fittings 1714 and 1718 and
outside surfaces of the wall 1710. Alternatively, the end fittings
1714 and 1718 may be securely engaged to the wall 1710 by
press-fitting, welding, brazing, etc. Each end fitting 1714 and
1718 includes a bore adapted for connection to the fluid lines of a
chromatographic system. For example, the bore may include threads
for engaging a fluid conduit fitting (not shown). Each bore is in
fluid communication with the column interior 1712 of the wall 1710,
whereby a fluid flow path is established from the first (inlet)
column end 1704 (inlet end), through the column interior 1712 and
to the second column end 1706 (outlet end).
The column interior 1712 extends from one axial end of the wall
1710 to the opposite axial end of the wall 1710. In the assembled
form of the column 1700, the column interior 1712 contains (is
filled with) a particulate packing material 1720 (only partially
shown) providing the stationary phase for chromatography. The
column 1700 includes frits (or filters) 1724 and 1726 configured to
serve as axial boundaries that retain the particles of the packing
material 1720 in place as a packed bed in the column interior 1712
while allowing fluid (e.g., a mobile phase/sample matrix) to flow
through the frits 1724 and 1726. The frits 1724 and 1726 may be
configured according to any of the embodiments disclosed herein,
for example the filter 500 described above and illustrated in FIGS.
5A-12B. The frits 1724 and 1726 may be positioned at each axial end
of the wall 1710. The column 1700 may also include respective frit
retainers 1732 and 1734 between the end fittings 1714 and 1718 and
frits 1724 and 1726. Each frit retainer 1732 and 1734 includes a
through-bore in fluid communication with the column interior 1712
via the corresponding frit 1724 and 1726, thereby fluidly
interconnecting the column interior 1712 and the bores of the end
fittings 1714 and 1718. The frit retainers 1732 and 1734 may
provide fluid-tight interfaces between the end fittings 1714 and
1718 and the fits 1724 and 1726. After loading the column interior
1712 with an appropriate amount of particulate material 1720,
assembly of the column 1700 may entail screwing or otherwise
securing the end fittings 1714 and 1718 onto the column 1700. Axial
movement of the end fittings 1714 and 1718 axially compresses the
end fittings 1714 and 1718 against the frit retainers 1732 and
1734, which in turn axially compresses the frit retainers 1732 and
1734 against the frits 1724 and 1726 and the frits 1724 and 1726
against the axial ends of the column wall 1710.
More generally, a filter as disclosed herein may be provided with
any type of fluid conduit. The filter may be mounted at or
integrated with the inlet end and/or outlet end of the conduit, or
at a point inside the conduit between the inlet and outlet ends.
The filter may be mounted to or integrated with a fluidic fitting
attached to the inlet or outlet end of the conduit. The fluidic
fitting may be of the type that provides a fluidly sealed
connection between the conduit and another conduit or fluidic
device.
FIG. 18 is a schematic view of an example of a fluidic system (or
liquid flow-based system) 1800 that may include one or more filters
as disclosed herein, for example any of the filters described above
and illustrated in FIGS. 5A-15. The fluidic system 1800 may include
various fluidic devices, for example fluidic devices 1804, 1808,
and 1852. In the present context, a "fluidic device" generally is a
device having a fluid inlet and/or a fluid outlet, and which
defines one or more liquid flow paths communicating with the fluid
inlet and/or fluid outlet. The fluidic device is configured to
perform one or more specific functions on liquid in the flow
path(s) of the fluidic device. The fluidic system 1800 may also
include various fluid lines communicating with (e.g., fluidly
coupled to) the fluid inlets and/or fluid outlets of the fluidic
devices, and in some cases providing an external liquid flow path
between two fluidic devices to enable liquid to be transferred from
one fluidic device to another fluidic device. In the illustrated
example, a fluid line 1826 communicates with the inlet of the
fluidic device 1804, a fluid line 1812 communicates with the outlet
of the fluidic device 1804 and the inlet of the fluidic device
1808, a fluid line 1854 communicates with the outlet of the fluidic
device 1808 and the inlet of the fluidic device 1852, and a fluid
line 1858 communicates with the outlet of the fluidic device
1852.
In various embodiments, one or more filters as disclosed herein may
be integrated with one or more of the fluidic devices 1804, 1808,
and 1852. Alternatively or additionally, one or more filters as
disclosed herein may be positioned in the flow path(s) of one or
more of the fluid lines 1826, 1812, 1854, and 1858.
In some embodiments, at least a part of the liquid flow path
provided by the fluidic system 1800 operates at high pressure. In
the present context, examples of "high pressure" include, but are
not limited to, a range of from 100 bar to 1500 bar or greater.
In one specific embodiment, the fluidic system 1800 is a liquid
chromatography (LC) system. In such an example, the fluidic device
1804 may be a pump, the fluidic device 1808 may be a
chromatographic column, and the fluidic device 1852 may be a
detector. Further, the fluid line 1826 may be a solvent supply
line, the fluid line 1812 may be a solvent delivery (or mobile
phase) line, the fluid line 1854 may be a column output line, and
the fluid line 1858 may be a detector output line. The design and
operation of various components of chromatography systems and other
types of fluid separation systems are generally known to persons
skilled in the art and thus need not be described in detail herein.
In one embodiment, a filter as disclosed herein may be utilized as
a frit in the chromatographic column, as described above and
illustrated in FIG. 17.
It will be understood that terms such as "communicate" and "in . .
. communication with" (for example, a first component "communicates
with" or "is in communication with" a second component) are used
herein to indicate a structural, functional, mechanical,
electrical, signal, optical, magnetic, electromagnetic, ionic or
fluidic relationship between two or more components or elements. As
such, the fact that one component is said to communicate with a
second component is not intended to exclude the possibility that
additional components may be present between, and/or operatively
associated or engaged with, the first and second components.
It will be understood that various aspects or details of the
invention may be changed without departing from the scope of the
invention. Furthermore, the foregoing description is for the
purpose of illustration only, and not for the purpose of
limitation--the invention being defined by the claims.
* * * * *